反应详情

34.8 g (0.1 mol) of 5-phenylsulphonyl-6-methyl-1,3-benzodioxole-2-carboxylic acid ethyl ester (from Example 2) are dissolved in 350 ml of dioxan (absolute) and treated in a pressure autoclave with approximately 20 g of ammonia gas. The reaction mixture is heated for 10 hours at 80° in the autoclave, the pressure is released, and the solution is concentrated to dryness by evaporation under reduced pressure. The residue is recrystallised from 120 ml of ethanol, yielding colourless crystals of 5-phenylsulphonyl-6-methyl-1,3-benzodioxole-2-carboxylic acid amide having a melting point of 138°-141°.

1. temperatureThe reaction mixture is heated for 10 hours at 80° in the autoclave
2. concentrationthe solution is concentrated to dryness by evaporation under reduced pressure
3. customThe residue is recrystallised from 120 ml of ethanol